CN113321217A - Preparation method of special high-dispersion white carbon black for high-ice-surface-gripping tire - Google Patents
Preparation method of special high-dispersion white carbon black for high-ice-surface-gripping tire Download PDFInfo
- Publication number
- CN113321217A CN113321217A CN202110735405.XA CN202110735405A CN113321217A CN 113321217 A CN113321217 A CN 113321217A CN 202110735405 A CN202110735405 A CN 202110735405A CN 113321217 A CN113321217 A CN 113321217A
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- CN
- China
- Prior art keywords
- carbon black
- white carbon
- sodium silicate
- reaction kettle
- electrolyte
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 239000006229 carbon black Substances 0.000 title claims abstract description 27
- 239000006185 dispersion Substances 0.000 title claims abstract description 9
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 26
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 26
- 239000002535 acidifier Substances 0.000 claims abstract description 14
- PHYFQTYBJUILEZ-IUPFWZBJSA-N triolein Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCC(OC(=O)CCCCCCC\C=C/CCCCCCCC)COC(=O)CCCCCCC\C=C/CCCCCCCC PHYFQTYBJUILEZ-IUPFWZBJSA-N 0.000 claims abstract description 13
- BAECOWNUKCLBPZ-HIUWNOOHSA-N Triolein Natural products O([C@H](OCC(=O)CCCCCCC/C=C\CCCCCCCC)COC(=O)CCCCCCC/C=C\CCCCCCCC)C(=O)CCCCCCC/C=C\CCCCCCCC BAECOWNUKCLBPZ-HIUWNOOHSA-N 0.000 claims abstract description 12
- PHYFQTYBJUILEZ-UHFFFAOYSA-N Trioleoylglycerol Natural products CCCCCCCCC=CCCCCCCCC(=O)OCC(OC(=O)CCCCCCCC=CCCCCCCCC)COC(=O)CCCCCCCC=CCCCCCCCC PHYFQTYBJUILEZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000003792 electrolyte Substances 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims description 31
- 239000000243 solution Substances 0.000 claims description 25
- 238000010438 heat treatment Methods 0.000 claims description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical group S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 239000008151 electrolyte solution Substances 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical group [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 6
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 6
- 235000011152 sodium sulphate Nutrition 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 229910052681 coesite Inorganic materials 0.000 claims description 2
- 229910052906 cristobalite Inorganic materials 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 229910052682 stishovite Inorganic materials 0.000 claims description 2
- 229910052905 tridymite Inorganic materials 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 3
- 230000001276 controlling effect Effects 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 229940117972 triolein Drugs 0.000 description 2
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- LRCFXGAMWKDGLA-UHFFFAOYSA-N dioxosilane;hydrate Chemical compound O.O=[Si]=O LRCFXGAMWKDGLA-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000012763 reinforcing filler Substances 0.000 description 1
- 229960004029 silicic acid Drugs 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004636 vulcanized rubber Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
Abstract
The invention discloses a preparation method of special high-dispersion white carbon black for a high-ice-surface-grip tire. The method comprises the following steps: and in the presence of electrolyte and glycerol trioleate, reacting sodium silicate with an acidifying agent to obtain the white carbon black. Compared with the existing white carbon black, the white carbon black prepared by the method can obviously improve the ice surface gripping force of the tire, effectively improve the safety of the tire when the tire runs on the ice surface, and ensure the driving safety under the weather condition in winter.
Description
Technical Field
The invention belongs to the field of white carbon black, and particularly relates to a preparation method of special high-dispersion white carbon black for a high-ice-surface-grip tire.
Background
The precipitated hydrated silica is commonly referred to as white carbon black, and is the most commonly used reinforcing filler in current tires. The white carbon black is a porous substance and has the advantages of high temperature resistance, non-combustion, tastelessness, odorless property and electrical insulation. With the increasing demand for green tires, high-quality white carbon black becomes a hot point for research. The improvement of the grip performance of the tire on the ice surface can effectively improve the safety of the tire when the tire runs on the ice surface and ensure the driving safety under the winter climate condition.
Disclosure of Invention
The invention aims to provide a preparation method of special high-dispersion white carbon black for a high-ice-surface-gripping tire.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of special high-dispersion white carbon black for a high-ice-surface-grip tire comprises the following steps: and in the presence of electrolyte and glycerol trioleate, reacting sodium silicate with an acidifying agent to obtain the white carbon black.
Preferably, the specific steps of the reaction are as follows:
(1) firstly, adding an electrolyte solution into a reaction kettle, and heating to 60-65 ℃;
(2) then adding a sodium silicate solution into the reaction kettle, adjusting the pH value to 9-10, and heating to 70-75 ℃;
(3) then glycerol trioleate is added into the reaction kettle;
(4) then adding a sodium silicate solution and an acidifying agent into the reaction kettle, controlling the pH value to be 10-11, and heating to 90-95 ℃ after the addition is finished;
(5) and continuously adding an acidifying agent, adjusting the pH value to 5-6, preserving heat, washing and drying to obtain the white carbon black.
Preferably, the electrolyte is sodium sulfate.
Preferably, the acidifying agent is sulfuric acid or hydrochloric acid.
Preferably, the glycerol trioleate is used in an amount of SiO20.5-5 per mill of the weight of the sodium silicate.
Preferably, in the step (1), the electrolyte solution occupies 1/6-1/7 of the volume of the reaction kettle.
More preferably, the concentration of the electrolyte in the electrolyte solution is 5 wt%.
Preferably, in the step (4), when the volume of the reaction solution accounts for 2/3-3/4 of the volume of the reaction kettle, the sodium silicate solution is stopped to be added.
More preferably, the concentration of the sodium silicate solution is 10 to 30 wt%.
Preferably, in the step (5), the temperature for heat preservation is 90-95 ℃ for 0.1-1 hour.
Detailed Description
The present invention will be described in further detail with reference to preferred embodiments.
The preparation method of the special high-dispersion white carbon black for the high-ice-surface-grip tire comprises the following steps: and in the presence of electrolyte and glycerol trioleate, reacting sodium silicate with an acidifying agent to obtain the white carbon black.
The method comprises the following specific steps:
(1) firstly, adding an electrolyte solution into a reaction kettle, and heating to 60-65 ℃;
(2) then adding a sodium silicate solution into the reaction kettle, adjusting the pH value to 9-10, and heating to 70-75 ℃;
(3) then glycerol trioleate is added into the reaction kettle;
(4) then adding a sodium silicate solution and an acidifying agent into the reaction kettle, controlling the pH value to be 10-11, and heating to 90-95 ℃ after the addition is finished;
(5) and continuously adding an acidifying agent, adjusting the pH value to 5-6, preserving heat, washing and drying to obtain the white carbon black.
The Zeta potential of the crystal grains can be regulated and controlled by adding the electrolyte, so that the reaction of the sodium silicate and the acidifying agent is promoted.
As one of the preferable technical solutions of the present invention, the electrolyte is selected from sodium sulfate.
In some preferred embodiments of the present invention, in the step (1), the electrolyte solution is added in an amount of 1/6 to 1/7 of the volume of the reaction kettle.
In some more preferred embodiments of the present invention, the electrolyte solution is a 5 wt% sodium sulfate solution.
As one of the preferable technical proposal of the invention, the acidifier is selected from sulfuric acid or hydrochloric acid.
In some preferred embodiments of the present invention, the amount of triolein is controlled to sodium silicate (as SiO)2Calculated) 0.5 to 5 per thousand of the weight, specifically such as 0.5 per thousand, 0.8 per thousand, 1 per thousand, 1.5 per thousand, 2 per thousand, 3 per thousand, 4 per thousand, 5 per thousand. The triolein is easy to foam when the dosage is more than the dosage, thus influencing the operation, and the dosage is less than the dosage, thus the effect of reducing the agglomeration probability of crystal grains can not be achieved.
In some preferred embodiments of the invention, in the step (4), the sodium silicate solution is stopped to be added when the volume of the reaction solution accounts for 2/3-3/4 of the volume of the reaction kettle.
In some preferred embodiments of the present invention, the concentration of the sodium silicate solution is 10 to 30 wt%, specifically, 10%, 15%, 20%, 25%, 30%. When the sodium silicate solution is higher than the concentration range, the agglomeration probability of the white carbon black is obviously increased, and when the sodium silicate solution is lower than the concentration range, the energy conservation and consumption reduction of the post-treatment of the white carbon black slurry are not facilitated.
In some preferred embodiments of the present invention, in the step (5), the temperature is maintained at 90-95 ℃ for 0.1-1 hour.
In some preferred embodiments of the present invention, the stirring speed of the reaction kettle is controlled to be 60-100 rpm.
The white carbon black prepared by the method has the following properties:
BET is 100 to 130m2/g,
The dispersion grade is more than or equal to 9.5,
the loss factor tan delta @ 20 ℃ of the corresponding vulcanized rubber is more than or equal to 1.0.
Compared with the commercial white carbon black, the white carbon black disclosed by the invention can improve the average deceleration of the rubber tire on the ice ground by more than 20% under the same addition amount, and the ice surface gripping force is obviously improved.
Example 1
(1) Adding a sodium sulfate solution with the concentration of 5 wt% into the reaction kettle, wherein the volume of the sodium sulfate solution is 1/6 of the volume of the reaction kettle, starting a stirrer (60 revolutions per minute), and heating to 60-65 ℃;
(2) then adding a sodium silicate solution with the concentration of 20 wt% into the reaction kettle, adjusting the pH value of the system to 9-10, and heating to 70-75 ℃;
(3) then glycerol trioleate (CAS:122-32-7) is added into the reaction kettle, and the added amount is sodium Silicate (SiO)2Calculated) 1 per mill of the total addition;
(4) then adding a sodium silicate solution with the concentration of 20 wt% and a sulfuric acid solution with the concentration of 10 wt% into the reaction kettle, controlling the pH value of the system to be 10-11 in the adding process, stopping adding the sodium silicate after the reaction liquid reaches 2/3 of the volume of the reaction kettle, and heating to 90-95 ℃;
(5) continuously adding a 10 wt% sulfuric acid solution, adjusting the pH value of the system to 5-6, and reacting for 15 minutes in a heat preservation manner.
(6) And after the reaction is finished, carrying out filter pressing, washing, pulping and spray drying on the slurry to obtain the white carbon black.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of special high-dispersion white carbon black for a high-ice-surface-grip tire comprises the following steps: and in the presence of electrolyte and glycerol trioleate, reacting sodium silicate with an acidifying agent to obtain the white carbon black.
2. The method of claim 1, wherein: the method comprises the following specific steps:
(1) firstly, adding an electrolyte solution into a reaction kettle, and heating to 60-65 ℃;
(2) then adding a sodium silicate solution into the reaction kettle, adjusting the pH value to 9-10, and heating to 70-75 ℃;
(3) then glycerol trioleate is added into the reaction kettle;
(4) then adding a sodium silicate solution and an acidifying agent into the reaction kettle, controlling the pH value to be 10-11, and heating to 90-95 ℃ after the addition is finished;
(5) and continuously adding an acidifying agent, adjusting the pH value to 5-6, preserving heat, washing and drying to obtain the white carbon black.
3. The production method according to claim 1 or 2, characterized in that: the electrolyte is sodium sulfate.
4. The production method according to claim 1 or 2, characterized in that: the acidifying agent is sulfuric acid or hydrochloric acid.
5.The production method according to claim 1 or 2, characterized in that: the glycerol trioleate is used in an amount of SiO20.5-5 per mill of the weight of the sodium silicate.
6. The method of claim 2, wherein: in the step (1), the electrolyte solution accounts for 1/6-1/7 of the volume of the reaction kettle.
7. The method of claim 6, wherein: the concentration of the electrolyte in the electrolyte solution was 5 wt%.
8. The method of claim 2, wherein: and (4) stopping adding the sodium silicate solution when the volume of the reaction solution accounts for 2/3-3/4 of the volume of the reaction kettle.
9. The method of claim 2, wherein: the concentration of the sodium silicate solution is 10-30 wt%.
10. The method of claim 2, wherein: in the step (5), the temperature is kept at 90-95 ℃ for 0.1-1 hour.
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CN202110735405.XA CN113321217A (en) | 2021-06-30 | 2021-06-30 | Preparation method of special high-dispersion white carbon black for high-ice-surface-gripping tire |
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